US4753738A - Sludge conditioning process - Google Patents

Sludge conditioning process Download PDF

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Publication number
US4753738A
US4753738A US07/083,536 US8353687A US4753738A US 4753738 A US4753738 A US 4753738A US 8353687 A US8353687 A US 8353687A US 4753738 A US4753738 A US 4753738A
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United States
Prior art keywords
ppm
paint
detackifier
sludge
floc
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Expired - Fee Related
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US07/083,536
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Shu-Jen Huang
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ChampionX LLC
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Nalco Chemical Co
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Priority to US07/083,536 priority Critical patent/US4753738A/en
Assigned to NALCO CHEMICAL COMPANY reassignment NALCO CHEMICAL COMPANY ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: HUANG, SHU-JEN
Application granted granted Critical
Publication of US4753738A publication Critical patent/US4753738A/en
Priority to EP88307129A priority patent/EP0302704B1/en
Priority to DE8888307129T priority patent/DE3861647D1/en
Priority to ZA885780A priority patent/ZA885780B/en
Priority to JP63195918A priority patent/JPH01135589A/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/71—Paint detackifiers or coagulants, e.g. for the treatment of oversprays in paint spraying installations
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S210/00—Liquid purification or separation
    • Y10S210/902—Materials removed
    • Y10S210/917—Color
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S210/00—Liquid purification or separation
    • Y10S210/93—Paint detackifying

Definitions

  • the invention is in the field of conditioning sludges for dewatering. More particularly, the invention is a process for conditioning sludges produced from paint spray detackification programs in the automotive industry for the purpose of increasing their solids content.
  • a good detackification program should provide a good sludge dewatering capability.
  • Sludge landfill disposal regulations vary from state-to-state, however, a sludge containing high solids and minimum solids is essential for most landfill sites.
  • clay/amine detackifier has been used to detackify the paint and create a floc.
  • clay/polymer detackifiers/flocculants have been utilized.
  • paint detackifier/flocculants are present in the water that collects the paint overspray.
  • a sludge is produced which must be removed from the waste water. This sludge is used as landfill. To minimize transporation cost and landfill volume, it is highly desirable to dewater the sludge to create as high a solids content as possible.
  • acrylamide/dimethylamino ethylmethacrylate methylsulfate quat i.e. Am/DMAEM MSQ
  • this dewatering aid has had an RSV between 7 and 10 and is present in concentrations as low as 0.1 ppm to 50 ppm actives.
  • this polymer has worked well because it has a high cationic charge being about 31% cationic in nature. This high cationic charge has reacted with the overall negative charge of the clay/amine and/or the clay/polymer flocculants systems utilized in the past.
  • a process for dewatering paint booth detackification sludge comprising the steps of detackifying the paint with a melamine-formaldehyde, and PVA and styrene-acrylate detackifier;
  • the water conditioner has an RSV of at least 6 RSV and more preferably of between 7 ⁇ 10. RSV is determined using 0.1 grams polymer per 100 milliliters of water at 25° C. Preferably the water conditioner will be at least 20 mole % DMAEM MSQ and most preferably between 28-35 mole %.
  • a water conditioner dose of 0.1 ppm or more actives will be satisfactory. More preferably the dosage will be 0.3-2 ppm. The dosage is based on total waste water.
  • the chemical detackifier was added to the waste water collection system to form a detackified floc. Subsequent to floc formation, sludge was separated from the waste water. When that sludge was then pumped to filtering machinery, the water conditioner was added. Mixing occurred in the piping on the way to the filtration machinery.
  • the filtration process utilized was a "filter assisted by vacuum” such as provided by the Hoffman Vacu-Matic and the Pecormatics. However, any mechanical process for dewatering can be used.
  • Tables II and III utilized the "filter assist by vacuum” method.
  • the melamine-formaldehyde, polyvinyl alcohol, styrene-acrylate detackifier mixture was used prior to the addition of the water conditioner.
  • acrylamide/dimethylaminoethylmethacrylate quat is designated as a methylsulfate quat.
  • the salt does not have to be a sulfate salt it could be any other salt reasonably generated, such as for example the chloride, the bromide, and the like. The use of the designator then is intended to be equivalent to all the other salts specified.
  • ppm is defined to mean parts per million on an actives basis.
  • the water conditioner had an RSV of 7-10 and was approximately 31 mole% DMAEM.
  • the ratio of polyvinyl alcohol to melamine formaldehyde to styrene acrylate is preferably within the ratio of 0.7:2.4:1 to 1.32:4.5:1 on a weight ratio based on actives.
  • the initial dosage ideally will be within the range of 25 to 500 ppm. But a maintenance dosage within the range of from 12:1 to 40:1 paint to detackifier on an active weight basis.

Abstract

A method of conditioning sludge formed in paint spray booths, where the detackifier is a melamine-formaldehyde, polyvinyl alcohol and styrene-acrylate paint detackier by adding a water conditioner that includes acrylamide/dimethylaminoethylmethacrylate methylsulfate quat.

Description

FIELD OF THE INVENTION
The invention is in the field of conditioning sludges for dewatering. More particularly, the invention is a process for conditioning sludges produced from paint spray detackification programs in the automotive industry for the purpose of increasing their solids content.
BACKGROUND
In the automotive industry paint which does not adhere to the automobile must be removed from the paint spray booth. Generally, this overspray is collected in a waste water system where it is detackified. After detackification, the paint solids are separated from the waste water, filtered and dewatered. The filtered solids are then removed to landfill sites for disposal.
A good detackification program should provide a good sludge dewatering capability. Sludge landfill disposal regulations vary from state-to-state, however, a sludge containing high solids and minimum solids is essential for most landfill sites.
Historically, a clay/amine detackifier has been used to detackify the paint and create a floc. Alternatively, clay/polymer detackifiers/flocculants have been utilized.
These paint detackifier/flocculants are present in the water that collects the paint overspray. When the floc has formed, a sludge is produced which must be removed from the waste water. This sludge is used as landfill. To minimize transporation cost and landfill volume, it is highly desirable to dewater the sludge to create as high a solids content as possible.
We have utilized an acrylamide/dimethylamino ethylmethacrylate methylsulfate quat (i.e. Am/DMAEM MSQ) polymer composition as the waste water conditioner which serves as a dewatering aid. Typically, this dewatering aid has had an RSV between 7 and 10 and is present in concentrations as low as 0.1 ppm to 50 ppm actives.
Generally, this polymer has worked well because it has a high cationic charge being about 31% cationic in nature. This high cationic charge has reacted with the overall negative charge of the clay/amine and/or the clay/polymer flocculants systems utilized in the past.
NEW DEVELOPMENTS
Recently, we have developed an all organic mixture of melamine-formaldehyde, polyvinyl alcohol, and styrene acrylate (i.e. melamine-formaldehyde, PVA, styrene acrylate) flocculants which act as paint detackifiers. These compositions are described in copending application Ser. No. 061,833 filed June 12, 1987 having the title "Paint Detackification" with the inventor, Shu-Jen Huang. This patent application is incorporated herein by reference.
Because of the overall composition of these paint detackifiers it was expected that the compositions create a floc which was substantially positive in character. For that reason, it was believed that the highly positive standard acrylamide/dimethylaminoethylmethacrylate methylsulfate quat dewatering compositions used with the prior clay/amine or clay/polymer detackifiers/flocculants would not work. For this reason, studies were conducted to find a suitable water conditioner for use as a dewatering aid.
SUMMARY OF THE INVENTION
Surprisingly, I have found that the positively charged acrylamide/dimethylaminoethylmethacrylate methylsulfate quat conditioning aid used for the negatively charged clay/amine and clay/polymer flocculant/detackifiers worked better with what was thought to be the positively charged melamine-formaldehyde, styrene-acrylate, and PVA paint detackifier mixtures and the flocs formed therefrom.
A process for dewatering paint booth detackification sludge comprising the steps of detackifying the paint with a melamine-formaldehyde, and PVA and styrene-acrylate detackifier;
Forming a detackified paint floc;
Adding an acrylamide/dimethylaminoethylmethacrylate methylsulfate quat water conditioner to the floc to form a sludge; and
Dewatering said sludge.
Generally the water conditioner has an RSV of at least 6 RSV and more preferably of between 7∝10. RSV is determined using 0.1 grams polymer per 100 milliliters of water at 25° C. Preferably the water conditioner will be at least 20 mole % DMAEM MSQ and most preferably between 28-35 mole %.
Generally a water conditioner dose of 0.1 ppm or more actives will be satisfactory. More preferably the dosage will be 0.3-2 ppm. The dosage is based on total waste water.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
A laboratory comparison of clay/polymer; clay/amine; and melamine/formaldehyde, polyvinyl alcohol, styrene-acrylate detackifiers was made. Each of the systems sludge was dewatered utilizing as a water conditioner acrylamide/dimethylaminoethylmethacrylate methylsulfate quat. The results are provided below:
              TABLE I                                                     
______________________________________                                    
                                Melamine-                                 
            Clay/               Formaldehyde                              
Chemical Program                                                          
            Polymer   Clay/Amine                                          
                                Styrene-Acrylate                          
______________________________________                                    
Total sludge                                                              
            80 cu     20 cu     15 cu yd/week                             
Production  yd/week   yd/week                                             
Sludge solids                                                             
            20%       40%       55%                                       
% Sludge Removal                                                          
            40%       80%       95%                                       
% Sludge Settling                                                         
            60%       20%        5%                                       
Pit cleaning                                                              
            Every     Every     Once a year                               
frequency   2 months  6 months                                            
Microbial   Heavy     Some      Minimum                                   
Control                                                                   
Foam control                                                              
            Heavy     Some      Minimum                                   
______________________________________
For each of the above tests, the chemical detackifier was added to the waste water collection system to form a detackified floc. Subsequent to floc formation, sludge was separated from the waste water. When that sludge was then pumped to filtering machinery, the water conditioner was added. Mixing occurred in the piping on the way to the filtration machinery. The filtration process utilized was a "filter assisted by vacuum" such as provided by the Hoffman Vacu-Matic and the Pecormatics. However, any mechanical process for dewatering can be used.
A series of tests were conducted at an existing automotive paint spray application facility. The following Table II provides a synopsis of the data collected:
              TABLE II                                                    
______________________________________                                    
                         BTU/lb                                           
%     %      BTU/lb.     of Dry Am/DMAEM MSQ                              
Solids                                                                    
      Ash    of Wet Sludge                                                
                         Sludge Active                                    
______________________________________                                    
32    12     3,684       10,960 0.155 ppm-0.31 ppm                        
20    16     3,800       10,420 0.155 ppm-0.31 ppm                        
40    8.9    5,385       11,460 0.155 ppm-0.31 ppm                        
31.9  14.9   3,740       10,720 0.155 ppm-0.31 ppm                        
36.3  8.3     4,0155     11,430 0.155 ppm-0.31 ppm                        
40.6  12.5   4,170       11,210 0.155 ppm-0.31 ppm                        
53    12     6,080       --      .sup. 0.775-1.55 pm                      
______________________________________
Additional data from another automotive paint spray booth waste water collection system is provided below in Table III:
              TABLE III                                                   
______________________________________                                    
                            Am/DMAEM MSQ                                  
%     %      BTU/lb.        70-100 ppm                                    
Solids                                                                    
      Ash    of Wet Sludge  As Active                                     
______________________________________                                    
51    1      7,490    RK-3840 "                                           
43    11     8,940    2 K Clear                                           
                              "                                           
36    8      6,110    WBE     "                                           
______________________________________                                    
 RD-3840 is a DuPont acrylic malamineformaldehyde resin used as a Clear   
 Coat.                                                                    
 2K  Clear is a two component isocyanate urethane Clear Coat.             
 WBE  is a white base enamel coating used in conjunction with either RK384
 or 2K Clear.
The data generated in Tables II and III utilized the "filter assist by vacuum" method. For each of those Tables, the melamine-formaldehyde, polyvinyl alcohol, styrene-acrylate detackifier mixture was used prior to the addition of the water conditioner.
Laboratory studies were conducted for the water conditioning aid. These studies are presented in Table IV below:
                                  TABLE IV                                
__________________________________________________________________________
        1A   1B   2A   2B   3A   3B                                       
__________________________________________________________________________
DMAEM-MSQ                                                                 
        16 ppm                                                            
             29 ppm                                                       
                  51 ppm                                                  
                       29 ppm                                             
                            94 ppm                                        
                                 53 ppm                                   
Paint   5453 ppm                                                          
             5776 7538 7538 10624                                         
                                 8122                                     
Sprayed                                                                   
Sludge  56.1 46   62   45.5 57   38                                       
% Solids                                                                  
Ratio of                                                                  
        0.29%                                                             
             0.50%                                                        
                  0.68%                                                   
                       0.51%                                              
                            0.88%                                         
                                 0.63%                                    
Conditioner/                                                              
Paint                                                                     
Detackifiers                                                              
        300 ppm                                                           
             861 ppm                                                      
                  420 ppm                                                 
                       970 ppm                                            
                            445 ppm                                       
                                 1060 ppm                                 
Used                                                                      
__________________________________________________________________________
 A = Clear Coat. The clear coat is an acrylic melamineformaldehyde resin  
 designated by DuPont as RK3840.                                          
 B = Base Coat. The Base Coat is an acrylic/polyester/melamine resin sold 
 by DuPont as a high solids base coat having the DuPont designator        
 872AB839.                                                                
 C = Is a combination of A and B. That is the base Coat has been applied  
 and the Clear Coat has been applied so that both compositions are in the 
 waste water for detackification.
Although the acrylamide/dimethylaminoethylmethacrylate quat is designated as a methylsulfate quat. The salt does not have to be a sulfate salt it could be any other salt reasonably generated, such as for example the chloride, the bromide, and the like. The use of the designator then is intended to be equivalent to all the other salts specified.
The use of the term ppm is defined to mean parts per million on an actives basis.
For all of the data given in the Tables the water conditioner had an RSV of 7-10 and was approximately 31 mole% DMAEM.
THE DETACKIFIER
Generally the ratio of polyvinyl alcohol to melamine formaldehyde to styrene acrylate is preferably within the ratio of 0.7:2.4:1 to 1.32:4.5:1 on a weight ratio based on actives. The initial dosage ideally will be within the range of 25 to 500 ppm. But a maintenance dosage within the range of from 12:1 to 40:1 paint to detackifier on an active weight basis.

Claims (2)

Having described my invention, I claim as follows:
1. A method for conditioning waste water to improve the dewaterability of solids contained therein comprising the steps of forming a detackified paint utilizing an all-organic melamine-formaldehyde, polyvinyl alcohol and styrene acrylate detackifier mixture; forming a detackified paint floc; and adding a acrylamide/dimethylaminoethylmethacrylate methylsulfate quat as a dewatering aid for the floc.
2. The method of claim 1 wherein said detackifier is used at a maintenance dose within the weight range of 12:1 to 40:1 paint to detackifier actives; and at least 0.155 ppm dewatering aid is used.
US07/083,536 1987-08-07 1987-08-07 Sludge conditioning process Expired - Fee Related US4753738A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
US07/083,536 US4753738A (en) 1987-08-07 1987-08-07 Sludge conditioning process
EP88307129A EP0302704B1 (en) 1987-08-07 1988-08-02 Sludge conditioning process
DE8888307129T DE3861647D1 (en) 1987-08-07 1988-08-02 METHOD FOR CONDITIONING SLUDGE.
ZA885780A ZA885780B (en) 1987-08-07 1988-08-05 Sludge conditioning process
JP63195918A JPH01135589A (en) 1987-08-07 1988-08-05 Control of sludge

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JP (1) JPH01135589A (en)
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ZA (1) ZA885780B (en)

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4792364A (en) * 1987-06-12 1988-12-20 Nalco Chemical Company Paint detackification
DE3831421A1 (en) * 1987-08-11 1989-03-30 Waldmann John J Composition for the treatment of paint-containing effluent, and process for the preparation thereof
US4869829A (en) * 1988-06-29 1989-09-26 Nalco Chemical Company Process for separating solids with a keratin filter aid
US4904393A (en) * 1988-05-27 1990-02-27 W. R. Grace & Co.-Conn. Method for controlling overspray in paint spray booths
US4913825A (en) * 1988-05-27 1990-04-03 W. R. Grace & Co.-Conn. Method for controlling overspray in paint spray booths
US4948513A (en) * 1988-05-27 1990-08-14 W. R. Grace & Co.-Conn. Method for controlling overspray in paint spray booths
US5006261A (en) * 1988-12-21 1991-04-09 Nalco Chemical Company Paint detackification using water-dispersible polymeric latexes
US5024768A (en) * 1988-02-29 1991-06-18 Betz Laboratories, Inc. Organic polymer activator for detackification
US5116514A (en) * 1991-04-08 1992-05-26 Nalco Chemical Company Method for detackifying oversprayed paint
US5192449A (en) * 1991-04-08 1993-03-09 Nalco Chemical Company Method for detackifying oversprayed paint
US5215668A (en) * 1991-07-31 1993-06-01 Nalco Chemical Company Anionic and nonionic solution polymers for paint detackification
US5248440A (en) * 1992-01-30 1993-09-28 W. R. Grace & Co.-Conn. Paint spray booth treatment of waterborne coatings
US5298186A (en) * 1990-05-15 1994-03-29 W. R. Grace & Co.-Conn. Paint spray booth organic detackification treatment
EP0656372A1 (en) * 1991-10-31 1995-06-07 KOHJIN CO. Ltd. Sludge dehydrating agent
WO2020007602A1 (en) * 2018-07-03 2020-01-09 Henkel Ag & Co. Kgaa Use of polyvinyl alcohols in water-based carrier media for separating paint overspray

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4002490A (en) * 1975-02-20 1977-01-11 Nalco Chemical Company Paint spray booth chemical treatment
US4055495A (en) * 1974-12-19 1977-10-25 Nalco Chemical Company Formulation and application of alkaline zinc chloride compositions and detackification of paint spray booth wastes
US4067806A (en) * 1976-09-16 1978-01-10 Nalco Chemical Company Formulation and application of compositions for the detackification of paint spray booth wastes
US4554026A (en) * 1982-06-21 1985-11-19 Nalco Chemical Company Aqueous hydrotrope solutions for paint detackifiers
US4686047A (en) * 1985-09-24 1987-08-11 Calgon Corporation Process for detackification of paint spray operation wastes

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4383927A (en) * 1982-03-08 1983-05-17 Nalco Chemical Company Recovery of oil from oily sludges
US4461866A (en) * 1982-05-24 1984-07-24 Sun Chemical Corporation Preparation of water-in-oil emulsions
GB8414950D0 (en) * 1984-06-12 1984-07-18 Allied Colloids Ltd Cationic polyelectrolytes
US4629572A (en) * 1986-02-27 1986-12-16 Atlantic Richfield Company Paint detackification method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4055495A (en) * 1974-12-19 1977-10-25 Nalco Chemical Company Formulation and application of alkaline zinc chloride compositions and detackification of paint spray booth wastes
US4002490A (en) * 1975-02-20 1977-01-11 Nalco Chemical Company Paint spray booth chemical treatment
US4067806A (en) * 1976-09-16 1978-01-10 Nalco Chemical Company Formulation and application of compositions for the detackification of paint spray booth wastes
US4554026A (en) * 1982-06-21 1985-11-19 Nalco Chemical Company Aqueous hydrotrope solutions for paint detackifiers
US4686047A (en) * 1985-09-24 1987-08-11 Calgon Corporation Process for detackification of paint spray operation wastes

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4792364A (en) * 1987-06-12 1988-12-20 Nalco Chemical Company Paint detackification
DE3831421A1 (en) * 1987-08-11 1989-03-30 Waldmann John J Composition for the treatment of paint-containing effluent, and process for the preparation thereof
DE3831421C2 (en) * 1987-08-11 1998-01-29 Waldmann John J A composition for treating waste water containing paint and varnish and process for their preparation
US5024768A (en) * 1988-02-29 1991-06-18 Betz Laboratories, Inc. Organic polymer activator for detackification
US4904393A (en) * 1988-05-27 1990-02-27 W. R. Grace & Co.-Conn. Method for controlling overspray in paint spray booths
US4913825A (en) * 1988-05-27 1990-04-03 W. R. Grace & Co.-Conn. Method for controlling overspray in paint spray booths
US4948513A (en) * 1988-05-27 1990-08-14 W. R. Grace & Co.-Conn. Method for controlling overspray in paint spray booths
US4869829A (en) * 1988-06-29 1989-09-26 Nalco Chemical Company Process for separating solids with a keratin filter aid
US5006261A (en) * 1988-12-21 1991-04-09 Nalco Chemical Company Paint detackification using water-dispersible polymeric latexes
US5298186A (en) * 1990-05-15 1994-03-29 W. R. Grace & Co.-Conn. Paint spray booth organic detackification treatment
US5116514A (en) * 1991-04-08 1992-05-26 Nalco Chemical Company Method for detackifying oversprayed paint
US5192449A (en) * 1991-04-08 1993-03-09 Nalco Chemical Company Method for detackifying oversprayed paint
EP0508605A1 (en) * 1991-04-08 1992-10-14 Nalco Chemical Company A method for detackifying oversprayed paint
US5215668A (en) * 1991-07-31 1993-06-01 Nalco Chemical Company Anionic and nonionic solution polymers for paint detackification
EP0656372A1 (en) * 1991-10-31 1995-06-07 KOHJIN CO. Ltd. Sludge dehydrating agent
EP0656372A4 (en) * 1991-10-31 1996-01-03 Kohjin Co Sludge dehydrating agent.
US5525692A (en) * 1991-10-31 1996-06-11 Kohjin Co., Ltd. Dewatering agent for sludge
US5248440A (en) * 1992-01-30 1993-09-28 W. R. Grace & Co.-Conn. Paint spray booth treatment of waterborne coatings
WO2020007602A1 (en) * 2018-07-03 2020-01-09 Henkel Ag & Co. Kgaa Use of polyvinyl alcohols in water-based carrier media for separating paint overspray

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EP0302704A2 (en) 1989-02-08
EP0302704A3 (en) 1989-05-03
ZA885780B (en) 1989-06-28
DE3861647D1 (en) 1991-02-28
JPH01135589A (en) 1989-05-29
EP0302704B1 (en) 1991-01-23

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